CN105339303B - The method for running fluidized-bed reactor - Google Patents
The method for running fluidized-bed reactor Download PDFInfo
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- CN105339303B CN105339303B CN201480035962.9A CN201480035962A CN105339303B CN 105339303 B CN105339303 B CN 105339303B CN 201480035962 A CN201480035962 A CN 201480035962A CN 105339303 B CN105339303 B CN 105339303B
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- gas
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- trichlorosilane
- purged
- purging
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- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000010926 purge Methods 0.000 claims abstract description 63
- 239000011261 inert gas Substances 0.000 claims abstract description 23
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 239000007789 gas Substances 0.000 claims description 83
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 claims description 21
- 239000005052 trichlorosilane Substances 0.000 claims description 21
- 239000012530 fluid Substances 0.000 claims description 19
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 17
- 229910052710 silicon Inorganic materials 0.000 claims description 16
- 239000010703 silicon Substances 0.000 claims description 16
- 239000001257 hydrogen Substances 0.000 claims description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000012495 reaction gas Substances 0.000 claims description 5
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims description 4
- 230000009466 transformation Effects 0.000 claims description 4
- 101000911390 Homo sapiens Coagulation factor VIII Proteins 0.000 claims description 3
- 102000057593 human F8 Human genes 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229940047431 recombinate Drugs 0.000 claims description 3
- 150000004756 silanes Chemical class 0.000 abstract description 11
- 206010037544 Purging Diseases 0.000 description 16
- 235000013339 cereals Nutrition 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 8
- 229910052698 phosphorus Inorganic materials 0.000 description 8
- 239000011574 phosphorus Substances 0.000 description 8
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 7
- 239000005046 Chlorosilane Substances 0.000 description 7
- 229910052796 boron Inorganic materials 0.000 description 7
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 7
- 239000002245 particle Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 230000008021 deposition Effects 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- 229910052734 helium Inorganic materials 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000011010 flushing procedure Methods 0.000 description 3
- 239000006260 foam Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 125000001475 halogen functional group Chemical group 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 239000011856 silicon-based particle Substances 0.000 description 2
- 238000009491 slugging Methods 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 235000011868 grain product Nutrition 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
- C01B33/10742—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material
- C01B33/10757—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material with the preferential formation of trichlorosilane
- C01B33/10763—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material with the preferential formation of trichlorosilane from silicon
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
- C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
- C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
- C01B33/03—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition of silicon halides or halosilanes or reduction thereof with hydrogen as the only reducing agent
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
- C01B33/10742—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material
- C01B33/10757—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material with the preferential formation of trichlorosilane
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The present invention provides a kind of method for running fluidized-bed reactor, including：Purging a is carried out to reactor and appendix with inert gas；Purging b is carried out to reactor and appendix with H2；With halogenated silanes or the mixture containing halogenated silanes carries out purging c to reactor and appendix.
Description
The present invention relates to a kind of method for running fluidized-bed reactor.
Fluidized-bed reactor by the reaction of HCl and metalluragical silicon at 350-400 DEG C for example for preparing trichlorosilane
(TCS).Equally can be in a fluidized bed reactor by containing STC/H2The metalluragical silicon manufacture TCS of (STC is silicon tetrachloride).
Fluidized-bed reactor is also used for the manufacture of polycrysalline silcon.This is achieved as follows：By the air-flow in fluid bed
Silicon grain is fluidized, the fluid bed is then heated to high temperature by heater.Add siliceous reacting gas as a result, in heat
Particle surface carries out pyrolytic reaction.Elemental silicon is deposited on silicon grain and individual particle is diametrically increasing.By regular
Take out the particle grown up and add less silicon grain as seed grain (hereinafter referred to as " seed "), methods described has
All related advantages and continuously operating.Described siliceous reacting gas refer to silicon-halogen compounds (such as：Chlorosilane
Or bromo-silicane), monosilane (SiH4), and the mixture of these gases and hydrogen.For example, this is disclosed by the A of US 4786477
Class deposition process and its equipment.
In the disassembling and recombinate of fluidized-bed reactor, oxygen and air humidity are entered in reactor by the atmosphere of surrounding
In portion and the pipeline that must be open.
The B2 of US 8017024 disclose a kind of method for being used to manufacture polycrysalline silcon in a fluidized bed reactor.Heavy
After product terminates, inside reactor is cooled down, while purged with inert gas, such as H2、N2, Ar, He or described gas mixing
Thing.Then, the silicon grain of cooling is discharged, disassembles reactor, reactor tube is substituted with new pipe, recombining reaction device, then by silicon
Particle is incorporated into reactor tube.Then, silicon grain is heated, starts new deposition operation.
The B2 of US 6827786 also illustrate a kind of fluidized-bed reactor.The purpose is to all low with carbon and oxygen impurities content
Gas contacts particle, thus recovers energy.
The purpose of the present invention is drawn by described problem.
The purpose is realized by a kind of method for running fluidized-bed reactor, and this method includes：Use indifferent gas
Body carries out purging a to reactor and appendix；Purging b is carried out to reactor and appendix with H2；With halogenated silanes or containing halo
The mixture of silane carries out purging c to reactor and appendix.
Preferably, H is used2While purging, temperature is heated to 100 to 1000 DEG C.
Preferably, the order of purge operation is a-b-c, i.e., is purged with inert gas, then blown with H2, first
Wash, then the mixture with halogenated silanes or containing halogenated silanes purges to it, then the deposit polycrystalline silicon on seed grain,
Reacting gas contains halogenated silanes.
Preferably, reacting gas is deposited on the kind crystalline substance of silicon in fluid bed, the high-purity for thus manufacturing the present invention is more
Crystal silicon particle.
Described reacting gas is preferably made up of the mixture of hydrogen and halogenated silanes, more preferably by hydrogen and trichlorosilane
Mixture composition.
It is preferred that fluidized-bed temperature is deposited in the case of being 700 DEG C to 1200 DEG C in conversion zone.
Initial fill of kind is brilliant in fluid bed is preferably fluidized by not siliceous fluidizing gas (preferably hydrogen), and is borrowed
Heat radiation is helped to be heated.
Described heat energy is uniformly introduced preferably by girth of the bidimensional radiator along fluid bed.
In conversion zone, because CVD reacts, siliceous reacting gas is deposited on silicon grain in the form of elemental silicon.
Unreacted reacting gas, fluidizing gas and gaseous state byproduct of reaction are discharged from reactor.
By regularly taking out the particle with deposition silicon from fluid bed, and crystal seed is added, methods described is sustainable
Run on ground.
The temperature of fluid bed in conversion zone is more preferably 850 DEG C to 1100 DEG C, most preferably 900 DEG C to 1050 DEG C.
Described reacting gas is preferably injected into fluid bed by one or more nozzles.
Absolute pressure in fluid bed is preferably between 0.1MPa and 1.1MPa, more preferably in 0.15MPa and 0.7MPa
Between, most preferably between 0.2MPa and 0.5MPa.
Based on the amount of all gases transported by fluid bed, the concentration of the siliceous reacting gas is preferably 10mol%
To 50mol%, more preferably 15mol% to 40mol%.
Based on the amount of all gases transported by reaction gas nozzle, the siliceous reacting gas in reaction gas nozzle
Concentration is preferably 20mol% to 50mol%.
Mean residence time of the reacting gas in fluid bed is preferably 100ms to 10s, more preferably 150ms to 5s, special
You Xuanwei not 200ms to 2s.
Fluid bed goes to run preferably as the fluid bed for forming foam.It is preferred that by some measures, for example, the selection height of bed and
The minimum ratio of bed diameter (plane bed), or mechanical foam destroyer is set in fluid bed, thus avoid slugging (slugging)
Operational mode, i.e., foam the diameter of fluid bed is grown in fluid bed, then the fluid bed material of compacting is pushed up, such as
It is the same with solid plug, until bubble collapse.
Preferably, in the case where reacting gas includes halogenated silanes, on seed grain after deposit polycrystalline silicon, terminate
The supply of the gas of silane reaction containing halo, purge operation b-a is then carried out, i.e., is purged, first with H2, then uses indifferent gas
Body is purged, and is then opened and is disassembled reactor.
Preferably, between the disassembling and recombinate of reactor, reactor and appendix are carried out further with inert gas
Purging.
Preferably, one or more of purging a, b, c are strengthened by transformation purging.
Preferably, the inert gas is nitrogen or rare gas, such as helium or argon gas.
Before with halogenated silanes/hydrogen mixture starting, the invention provides the inerting of reactor.This is initially used for being avoided
Hydrogen oxygen gas burst；Next avoid as moisture or the impurity as caused by moisture to polycrysalline silcon product pollution (such as：Come
From the phosphorus of steel).It has been found that the purge operation of the present invention is substantially more more effective than step known in the art.
When reactor shuts down, it is also advantageous to make wherein to be sent into halogenated silanes/hydrogen mixture by inerting
Stage is separated with first switching on reactor, because otherwise reacting gas can be discharged into the external world.
Therefore, purged (upon start up) with inert gas and then with hydrogen, or purged with hydrogen and then with inert gas (when
During stopping), available for before deposition afterwards by reaction condition and external condition separation.
The halogenated silanes is preferably chlorosilane, particularly preferably using trichlorosilane.
Between the appropriate stage, it is determined that volume flow rate under, the purge operation of time is determined with inert gas,
Thus inerting can be implemented.
Upon start up, purged first with inert gas, then fill reactor with trichlorosilane/hydrogen mixture.
When stopping, after trichlorosilane/hydrogen feed is closed, purged with inert gas, then opened first
Reactor.
Special advantage of the invention is：
- with check operation curve establish inert condition；
Any explosive mixture of-prevention；
- reduce pollution of the entrance to product due to moisture.
One special advantage is：With inert gas purge additionally reducing and caused with the moisture of seed grain introducing
Pollution.
In purge operation, the volume of pipeline and reactor is all crucial for flushing times and purge gas volume.
In addition, the desired level of the silicon grain product quality manufactured during later deposition also influences flushing times and purge gas body
Product.Therefore, can be longer for the flushing times needed for the high purity product of semi-conductor industry compared to for field of solar energy.
Preferable starting step：
1. purge operation a：With inert gas (N2, Ar, He) it is determined that reactor and appendix are purged in the time, with discharge
O2 and moisture.
Purge operation a is carried out 0.5 to 10 hour.Run and heated for the gas of fluidizing gas and reacting gas at room temperature
Device.It is 10 to 500Nm in purge gas speed3/h(m3(STP)/h) under purged, the purge gas by 100% indifferent gas
Body forms, such as nitrogen.
2. purge operation b：With H2 it is determined that time in purge reactor and appendix, to discharge inert gas.
Purge operation b is carried out 2 to 100 hours.Gas heater is run at being 100 to 1000 DEG C in temperature.In purging gas
Body speed is 200 to 1000Nm3Purged under/h, the purge gas is made up of 100% hydrogen.
3. purge operation c：Under constant superficial gas speed, H2 is exchanged in opposite slope (opposite ramp)
For trichlorosilane or trichlorosilane mixture.
Purge operation c is carried out 2 to 50 hours.The purge gas speed set herein will meet following standard：
Based on the amount of all gases transported by fluid bed, the concentration of the siliceous reacting gas is preferably 10mol%
To 50mol%, more preferably 15mol% to 40mol%.
Based on the amount of all gases transported by reaction gas nozzle, the siliceous reacting gas in reaction gas nozzle
Concentration is preferably 20mol% to 50mol%.
Therefore, purged with identical gas volume used during deposition.The particle deposited during this period is downgraded to not
Qualified material.Gas heater is run at being 100 to 1000 DEG C in temperature.Open reactor heaters.
Purging can be lasting or can be purged by transformation to strengthen.
It is preferable to stop step：
1. close the supply of chlorosilane；
2. purge operation b：Reactor and appendix are purged with H2.Purge operation b is carried out 1 to 20 hour.Gas heater
Run at a temperature of 100 to 1000 DEG C.It is 50 to 800Nm in purge gas speed3Purged under/h.
3. inerting is carried out to reactor and appendix with inert gas (N2, Ar, He).It is small that purge operation a carries out 1 to 20
When.Gas heater is run at room temperature.It is 10 to 500Nm in purge gas speed3Purged under/h.
4. the opening of equipment and disassemble
Purging can also be purged to strengthen by transformation.
When changing batch, shutdown purging can also be carried out with inert gas.
For this purpose, purge all pipelines for leading to reactor and the pipeline for leaving reactor with inert gas.Purge gas
Body speed is at room temperature in 1 and 500Nm3Between/h.
If reactor without starting at once, carries out shutdown purging in the assembled condition in the reassembled.This is included with lazy
Property gas, using purge gas speed as 1 to 500Nm3/ h, purge all pipelines for leading to and leaving reactor and reactor sheet
Body.The measure prevents forms incrustation in downtime.When discharging remaining compound from dead space or pipe arm, such as due to
Corrosion may produce incrustation.This quality to product has detrimental effect.
By Fig. 1 and 2, the present invention will be described in detail below.
Brief description of the drawings
Fig. 1 shows the ratio of inert gas, H2 and chlorosilane air-flow during startup relative to the curve of time.
Fig. 2 shows the ratio of inert gas, H2 and chlorosilane air-flow during stopping relative to the curve of time.
Fig. 1 is shown only carries out several hours purgings with inert gas first.Then it is several that H2 progress is similarly only used only
Individual hour purging.Thereafter, chlorosilane is added into H2 air-flows, to reach above-mentioned concentration.
Fig. 2 is shown stops supply chlorosilane first, improves H2 supply and only with H2 purge within several hours.This
Afterwards, only purged with inert gas, be similarly several hours.
Embodiment
In purge operation b, purging is carried out 2 hours to the reactor that internal diameter is 400mm.Gas velocity is 600Nm3/h；
It will be 500 DEG C for the temperature setting of reacting gas and the gas heater of fluidizing gas.The virgin curve of phosphorus and boron dope agent
It is relatively blunt so that phosphorus pollution can only be made after reactor is run 2 weeks<800ppta and boron pollution<50ppta highest
Quality material.This material is applied to field of solar energy, rather than semiconductor applications.
In purge operation b, purging is carried out 30 hours to the reactor that internal diameter is 400mm.Gas velocity is 600Nm3/h；
It will be 100 DEG C for the temperature setting of reacting gas and the gas heater of fluidizing gas.The virgin curve of phosphorus and boron dope agent
It is blunt so that phosphorus pollution can only be made after reactor is run 1.5 weeks<800ppta and boron pollution<50ppta is most
High quality material.This material is applied to field of solar energy, rather than semiconductor applications.
In purge operation b, purging is carried out 30 hours to the reactor that internal diameter is 400mm.Gas velocity is 200Nm3/h；
It will be 500 DEG C for the temperature setting of reacting gas and the gas heater of fluidizing gas.The virgin curve of phosphorus and boron dope agent
It is blunt so that phosphorus pollution can only be made after reactor is run 2 weeks<800ppta and boron pollution<50ppta highest
Quality material.This material is applied to field of solar energy, rather than semiconductor applications.
In purge operation b, purging is carried out 30 hours to the reactor that internal diameter is 400mm.Gas velocity is 600Nm3/h；
It will be 500 DEG C for the temperature setting of reacting gas and the gas heater of fluidizing gas.Only after operation 2 days, obtain pair
In the first-chop material of semi-conductor industry, the pollution of its phosphorus<200ppta and boron pollution<30ppta.
Claims (8)
1. one kind is by silicon and HCl or by silicon and H2/ tetrachloro silicane is prepared in the operation of trichlorosilane, or by trichlorosilane system
For the method in the operation of silicon, running fluidized-bed reactor, including：At room temperature 10 to 500Nm in (a) is purged3/ h's
Reactor and appendix purge 0.5 to 10 hour with inert gas under gas flow rate；Then with by gas in (b) is purged
Body heater is heated to 100-1000 DEG C of H2Reactor and appendix are purged, wherein it is described purging with 200 to
1000Nm3/ h gas flow rate is carried out 2 to 100 hours；And then in (c) is purged it is heated to 100- with by gas heater
1000 DEG C of trichlorosilane or mixture containing trichlorosilane carry out purging to reactor and appendix 2 to 50 hours, use this
The amount of the purge gas of sample so that the amount based on total gas by fluid bed, trichlorosilane or trichlorosilane mixture it is dense
It is 10mol% to 50mol% to spend, and the amount based on total gas by reaction gas nozzle, the trichlorosilane or described
The concentration of trichlorosilane mixture is 20mol% to 50mol%.
2. according to the method for claim 1, wherein after the purge operation according to (a)-(b)-(c) orders, by containing
The reacting gas of trichlorosilane, the deposit polycrystalline silicon on seed grain.
3. according to the method for claim 2, wherein the reacting gas includes hydrogen and trichlorosilane.
4. according to the method in any one of claims 1 to 3, be included in reacting gas include trichlorosilane in the case of,
The deposit polycrystalline silicon on seed grain, the supply of the reacting gas containing trichlorosilane is then terminated, in (b) is purged, with by gas
Body heater is heated to 100-1000 DEG C of H2The reactor and the appendix are purged, wherein the purging is with 50
To 800Nm3/ h gas flow rate is carried out 1 to 20 hour, and then at room temperature with 10 to 500Nm3/ h gas flow rate is with lazy
Property gas purging is carried out to the reactor and the appendix 1 to 20 hour, and then open and disassemble the reactor.
5. according to the method for claim 4, wherein the reactor is then recombinated, and add seed grain.
6. according to the method for claim 5, it is included between the disassembling and recombinate of the reactor, with inert gas to anti-
Device and appendix is answered further to be purged.
7. according to the method in any one of claims 1 to 3, wherein one or more purged in (a), (b), (c)
It is individual to be strengthened by transformation purging.
8. according to the method in any one of claims 1 to 3, wherein the inert gas is nitrogen or rare gas.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102013212406.6A DE102013212406A1 (en) | 2013-06-27 | 2013-06-27 | Method for operating a fluidized bed reactor |
| DE102013212406.6 | 2013-06-27 | ||
| PCT/EP2014/062661 WO2014206805A1 (en) | 2013-06-27 | 2014-06-17 | Method for operating a fluidized bed reactor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105339303A CN105339303A (en) | 2016-02-17 |
| CN105339303B true CN105339303B (en) | 2017-12-19 |
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ID=50943323
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201480035962.9A Expired - Fee Related CN105339303B (en) | 2013-06-27 | 2014-06-17 | The method for running fluidized-bed reactor |
Country Status (11)
| Country | Link |
|---|---|
| US (1) | US10526206B2 (en) |
| EP (1) | EP3013744B1 (en) |
| JP (1) | JP6178006B2 (en) |
| KR (1) | KR101842373B1 (en) |
| CN (1) | CN105339303B (en) |
| DE (1) | DE102013212406A1 (en) |
| ES (1) | ES2647501T3 (en) |
| MY (1) | MY170696A (en) |
| SA (1) | SA515370311B1 (en) |
| TW (1) | TWI526395B (en) |
| WO (1) | WO2014206805A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102016203082A1 (en) * | 2016-02-26 | 2017-08-31 | Wacker Chemie Ag | Process for depositing an in-situ coating on thermally and chemically stressed components of a fluidized bed reactor for producing high-purity polysilicon |
| CN109562951A (en) * | 2016-12-14 | 2019-04-02 | 瓦克化学股份公司 | The method for being used to prepare polysilicon |
| CN110049948B (en) * | 2016-12-14 | 2022-10-11 | 瓦克化学股份公司 | Method for preparing polycrystalline silicon |
| KR102607348B1 (en) * | 2018-12-18 | 2023-11-29 | 와커 헤미 아게 | How to make chlorosilane |
| CN115594184B (en) * | 2022-10-31 | 2023-10-10 | 唐山三孚硅业股份有限公司 | Electronic grade silicon tetrachloride production system and method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4416913A (en) * | 1982-09-28 | 1983-11-22 | Motorola, Inc. | Ascending differential silicon harvesting means and method |
| US4642228A (en) * | 1985-07-24 | 1987-02-10 | Angel Sanjurjo | Fluxing system for reactors for production of silicon |
| CN101400835A (en) * | 2006-06-15 | 2009-04-01 | 韩国化学研究院 | Method for continual preparation of polycrystalline silicon using a fluidized bed reactor |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4359490A (en) | 1981-07-13 | 1982-11-16 | Fairchild Camera & Instrument Corp. | Method for LPCVD co-deposition of metal and silicon to form metal silicide |
| KR880000618B1 (en) | 1985-12-28 | 1988-04-18 | 재단법인 한국화학연구소 | Preparation for silicon multy crystal |
| JP3737863B2 (en) * | 1996-11-26 | 2006-01-25 | 株式会社トクヤマ | Method for producing granular polysilicon |
| US6827786B2 (en) | 2000-12-26 | 2004-12-07 | Stephen M Lord | Machine for production of granular silicon |
| DE10203833B4 (en) | 2002-01-31 | 2007-02-08 | Siltronic Ag | Method and device for differential pressure control on epitaxy reactors |
| DE102006037020A1 (en) * | 2006-08-08 | 2008-02-14 | Wacker Chemie Ag | Method and apparatus for producing high purity polycrystalline silicon with reduced dopant content |
| US20100276002A1 (en) * | 2007-09-20 | 2010-11-04 | Nuofu Chen | Process and apparatus for producing polysilicon sheets |
| KR20130105618A (en) * | 2010-09-08 | 2013-09-25 | 다우 코닝 코포레이션 | Method for preparing a trihalosilane |
-
2013
- 2013-06-27 DE DE102013212406.6A patent/DE102013212406A1/en not_active Withdrawn
-
2014
- 2014-06-17 JP JP2016522390A patent/JP6178006B2/en not_active Expired - Fee Related
- 2014-06-17 CN CN201480035962.9A patent/CN105339303B/en not_active Expired - Fee Related
- 2014-06-17 EP EP14730539.5A patent/EP3013744B1/en not_active Not-in-force
- 2014-06-17 KR KR1020167002240A patent/KR101842373B1/en active IP Right Grant
- 2014-06-17 MY MYPI2015003011A patent/MY170696A/en unknown
- 2014-06-17 US US14/899,143 patent/US10526206B2/en not_active Expired - Fee Related
- 2014-06-17 ES ES14730539.5T patent/ES2647501T3/en active Active
- 2014-06-17 WO PCT/EP2014/062661 patent/WO2014206805A1/en active Application Filing
- 2014-06-18 TW TW103121005A patent/TWI526395B/en not_active IP Right Cessation
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4416913A (en) * | 1982-09-28 | 1983-11-22 | Motorola, Inc. | Ascending differential silicon harvesting means and method |
| US4642228A (en) * | 1985-07-24 | 1987-02-10 | Angel Sanjurjo | Fluxing system for reactors for production of silicon |
| CN101400835A (en) * | 2006-06-15 | 2009-04-01 | 韩国化学研究院 | Method for continual preparation of polycrystalline silicon using a fluidized bed reactor |
Also Published As
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| TWI526395B (en) | 2016-03-21 |
| TW201500280A (en) | 2015-01-01 |
| DE102013212406A1 (en) | 2014-12-31 |
| US10526206B2 (en) | 2020-01-07 |
| ES2647501T3 (en) | 2017-12-21 |
| JP2016530184A (en) | 2016-09-29 |
| JP6178006B2 (en) | 2017-08-09 |
| MY170696A (en) | 2019-08-26 |
| EP3013744A1 (en) | 2016-05-04 |
| CN105339303A (en) | 2016-02-17 |
| EP3013744B1 (en) | 2017-09-20 |
| US20160145109A1 (en) | 2016-05-26 |
| KR101842373B1 (en) | 2018-03-26 |
| KR20160022930A (en) | 2016-03-02 |
| WO2014206805A1 (en) | 2014-12-31 |
| SA515370311B1 (en) | 2017-06-27 |
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